WO2014104759A1 - Matériau actif de cathode pour batteries secondaires au lithium - Google Patents
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- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
- C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-x-y)O2
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- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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- C01P2006/11—Powder tap density
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- C01P2006/40—Electric properties
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the present invention relates to a cathode active material for a lithium secondary battery, and more particularly, to a cathode active material for a lithium secondary battery having improved tap density by mixing cathode active materials having different sizes, wherein at least one particle of the cathode active material to be mixed is particles. It relates to a cathode active material for a lithium secondary battery, characterized by having a concentration gradient within.
- the porosity of the electrode In the lithium secondary battery, it is necessary to maintain the porosity of the electrode above a certain level in consideration of the ion conductivity of the active material.
- the porosity of the electrode When the electrode is rolled at a high rolling rate to improve the loading amount or the electrode density, the porosity of the electrode is excessively reduced, causing a sharp decrease in the C-rate.
- An object of the present invention is to provide a cathode active material for a lithium secondary battery that can exhibit a good C-rate while reducing the porosity in order to solve the problems of the prior art as described above.
- the present invention in order to solve the above problems, in the positive electrode active material for a lithium secondary battery comprising a mixture of particles P1 having a diameter of D1, particles P2 having a diameter of D2, any one of the particles P1, the particles P2 is represented by the following formula It provides a positive electrode active material for a lithium secondary battery having a central portion represented by 1 and the surface portion represented by the following formula (2).
- M1, M2 and M3 are selected from the group consisting of Ni, Co, Mn, and combinations thereof
- M4 is Fe, Na, Mg, Ca, Ti, V, Cr, Cu, Zn, Ge , Sr, Ag, Ba, Zr, Nb, Mo, Al, Ga, B and combinations thereof, 0 ⁇ a1 ⁇ 1.1, 0 ⁇ a2 ⁇ 1.1, 0 ⁇ x1 ⁇ 1, 0 ⁇ x2 ⁇ 1, 0 ⁇ y1 ⁇ 1, 0 ⁇ y2 ⁇ 1, 0 ⁇ z1 ⁇ 1, 0 ⁇ z2 ⁇ 1, 0 ⁇ w ⁇ 0.1, 0.0 ⁇ 0.02, 0 ⁇ x1 + y1 + z1 ⁇ 1, 0 ⁇ x2 + y2 + z2 ⁇ 1, x1 ⁇ x2, y1 ⁇ y2, z2 ⁇ z1.)
- the present invention consists of a mixture of particles of positive electrode active material having different sizes, which is composed of a mixture of particles having a constant concentration of metal ions in the particles and particles having different compositions in the center and surface portions in the particles, or in the particles in the center and surfaces. It relates to a positive electrode active material composed of a mixture of particles having a different composition.
- a positive electrode active material composed of a mixture of particles having a different composition.
- the particle P1 has a central portion represented by the formula (1) and a surface portion represented by the formula (2), the diameter D1 of P1 and the diameter D2 of P2 are 2 to 20 ⁇ m, satisfying the relationship of D1 ⁇ D2
- the particles P1 may be included in a ratio of 5 to 95 parts by weight based on 100 parts by weight of the total positive electrode active material.
- the particle having a large particle size and a constant metal concentration is filled. While the high power characteristics as a whole, the particle size is small, the composition of the thermal stability is improved by the particles having different compositions of the central portion and the surface portion.
- the particle size is small and the particles having different compositions in the central portion and the surface portion are filled in the space between the particles having a large size and the composition in the central portion and the surface portion, high thermal stability and high capacity can be exhibited.
- the particle P1 has a central portion represented by the formula (1) and a surface portion represented by the formula (2), the diameter D1 of P1 and the diameter D2 of P2 are 2 to 20 ⁇ m, and the relationship of D2 ⁇ D1
- the particle P1 may be included in a ratio of 5 to 95 parts by weight based on 100 parts by weight of the total positive electrode active material.
- a structure in which particles having a small particle size and a constant metal concentration are filled in a space between particles having a large particle size and a different composition of the central portion and the surface portion While the thermal stability is improved by the particles as a whole, the particles having a small size and a constant metal concentration can exhibit high output characteristics.
- the positive electrode active material for the lithium secondary battery having different compositions of the center portion and the surface portion is not limited to the internal structure as long as the composition of the center portion and the surface portion is different. That is, the concentration of the metal constituting the positive electrode active material can form a continuous concentration gradient in the entire region from the center of the particle to the surface portion, or form a core-shell structure, a certain core, depending on the thickness of the central portion and the surface portion. Concentration gradients can then be formed only in the shell part.
- the thickness of the central portion is 10 to 70% of the total size of the cathode active material particles for lithium secondary battery,
- the concentration of the metal ions from the central portion to the surface portion is represented by the formula (2), that is, characterized in that the core and shell structure having a constant concentration.
- the central portion occupies 10 to 70% of the distance from the center of the particle to the outermost surface, and 90 to 30% of the distance.
- the surface portion occupies. If the ratio of the center portion is 70% or more of the distance from the center of the aperture to the outermost surface, the surface portion is too thin to cover the surface of the uneven aperture, and the ratio of the center portion of the aperture is the center of the aperture. If it is 10% or less of the distance from the outermost surface to the outermost surface, the charge / discharge capacity of the center portion may be lowered and the capacity accompanying the cycle may be lowered.
- the thickness of the central portion is 10 to 70% of the total size of the cathode active material particles for lithium secondary battery,
- the thickness of the surface portion is 1 to 5% of the total size of the cathode active material particles for lithium secondary battery
- the concentration of M1, M2, and M3 have a continuous concentration gradient from the central portion to the surface portion.
- the central portion and the thickness of the surface portion is 1 to 5% of the total size of the cathode active material particles for lithium secondary battery
- the concentration of M1, M2, and M3 have a continuous concentration gradient from the central portion to the surface portion.
- the cathode active material for a lithium secondary battery having a central portion represented by Chemical Formula 1 and a surface portion represented by Chemical Formula 2 of the present invention increases the concentration of M1 and M2 with a continuous concentration gradient from the central portion to the surface portion,
- the concentration of M3 is characterized in that it decreases with a continuous concentration gradient toward the surface portion from the central portion.
- the concentrations of M1 and M2 are continuous from the center portion to the surface portion.
- the concentration increases with a concentration gradient, and the concentration of M3 decreases with a continuous concentration gradient from the center to the surface portion.
- the concentration distribution means that there is a difference of 0.05 to 15 mol%, preferably 0.05 to 10 mol%, more preferably 0.05 to 5 mol%, of a change in metal concentration per 0.1 ⁇ m from the center of the particle to the surface portion.
- one or more concentration gradient slopes may be included throughout the particles, specifically, the concentration of the metal in the entire region from the particle center to the surface may be particles having one continuous concentration gradient slope, or particles The concentration of metal in the region from the center to the surface may be particles having two or more different concentration gradient gradients.
- the central portion and the thickness of the surface portion is 1 to 5% of the total size of the cathode active material particles for lithium secondary battery
- the concentration of M1 is constant from the central portion to the surface portion
- the concentration of M2 and the concentration of M3 toward the surface portion from the central portion is characterized by having a continuous concentration gradient.
- M1 is Co
- M2 is Mn
- M3 is characterized in that Ni.
- M1 is Mn
- M2 is Co
- M3 is characterized in that Ni.
- M1 is Ni
- M2 is Co
- M3 is characterized in that Mn.
- the present invention also provides an electrode including the cathode active material, a lithium secondary battery comprising the electrode.
- the cathode active material according to the present invention not only enhances the C-rate characteristics by mixing particles having different sizes, but also includes particles having a gradient of metal ions in the particles to be mixed, and also has appropriate porosity. By maintaining the positive electrode active material can be produced significantly improved tap density.
- Figure 1 shows the results of measuring the PSA according to the ratio of the particles mixed in the positive electrode active material according to an embodiment of the present invention.
- Figure 2 shows the tap density according to the proportion of the particles mixed in the positive electrode active material according to an embodiment of the present invention.
- 3 and 4 show the results of measuring the PSA of the positive electrode active material according to an embodiment of the present invention.
- an aqueous metal salt solution having a concentration of 2.0 M in which nickel sulfate, cobalt sulfate, and manganese sulfate is mixed in a molar ratio of 90: 5: 5 is used as an aqueous metal salt solution for forming a core.
- the metal salt aqueous solution for forming a core was first introduced into a reactor. Then, the mixture was mixed while gradually changing the mixing ratio of the aqueous metal salt solution for forming the center portion and the aqueous metal salt solution for forming the surface portion, and charged at a rate of 0.3 liters / hour. In addition, a 4.0 M concentration of ammonia solution was continuously added to the reactor at 0.03 liter / hour.
- a 4.0 M sodium hydroxide aqueous solution was supplied for pH adjustment to maintain pH at 10. Impeller speed was adjusted to 1000 rpm. The flow rate was adjusted so that the average residence time of the solution in the reactor was about 6 hours. After the reaction reached a steady state, a solution containing a cathode active material precursor for a lithium secondary battery was continuously obtained through an overflow pipe.
- the solution containing the obtained cathode active material precursor for lithium secondary batteries was filtered, washed with water, and dried in a 110 ° C. warm air dryer for 15 hours to prepare a cathode active material precursor for lithium secondary batteries.
- cathode active material precursor for lithium secondary batteries After mixing the prepared cathode active material precursor for lithium secondary batteries and lithium hydroxide (LiOH) in a molar ratio of 1.0: 1.19, and heated at a temperature increase rate of 2 °C / min, and maintained at 280 °C for 5 hours, preliminary baking was performed, Subsequently, the resultant was calcined at 900 ° C. for 10 hours to obtain a cathode active material for a lithium secondary battery having a particle size of 4 to 7 ⁇ m and a tap density of 1.97 g / cc, and a particle size of 10 to 14 ⁇ m and a tap density of 2.42 g / cc. Each of the measured cathode active materials for lithium secondary batteries was prepared.
- a cathode active material in which the concentration of Mn is fixed at 25% and the concentration of Co and Ni is gradient, 2.0, in which nickel sulfate, cobalt sulfate, and manganese sulfate were mixed in a molar ratio of 75:00:25 as an aqueous metal salt solution for forming a core.
- the metal salt for forming the center portion was first introduced into the reactor, except that the mixing rate of the metal salt aqueous solution for forming the center portion and the metal salt aqueous solution for forming the surface portion was gradually mixed and added at a rate of 0.3 liters / hour.
- the concentration of Mn is fixed at 25% and the concentration of Co and Ni is gradient as in 1, and the particle size is 4 to 6 ⁇ m and the tap density is 2.03 g / cc.
- a cathode active material having two or more concentration gradients of Mn, Co, and Ni 2.0 M concentration of nickel sulfate, cobalt sulfate, and manganese sulfate was mixed in a molar ratio of 80:05:15 as a metal salt aqueous solution for forming a core.
- An aqueous solution was prepared, and as an aqueous metal salt solution for forming the first surface portion, a 2.0 M metal solution in which nickel sulfate, cobalt sulfate, and manganese sulfate was mixed in a molar ratio of 70:10:20 was prepared, and the metal salt for forming the second surface portion was prepared.
- the aqueous metal salt solution for forming the core was first introduced into a reactor, and the core for forming the core was added thereto. After mixing at a constant rate while gradually changing the mixing ratio of the aqueous metal salt solution and the aqueous metal salt solution for forming the first surface portion, the first surface portion was introduced at a rate of 0.3 liters / hour.
- the size of the concentration gradient was the same as in Preparation Example 1, except that the mixing ratio of the aqueous metal salt aqueous solution and the aqueous metal salt aqueous solution for forming the second surface portion was gradually mixed and fed at a rate of 0.3 liter / hour.
- Cathode active material for lithium secondary batteries having a particle size of 6 ⁇ m and a tap density of 2.17 g / cc, and a cathode active material for lithium secondary batteries having a particle size of 10 to 14 ⁇ m and a tap density of 2.52 g / cc was prepared.
- a metal solution for forming a core having a concentration of 2.0 M in which nickel sulfate, cobalt sulfate, and manganese sulfate was mixed at a molar ratio of 95:00:05 was prepared, and for shell formation
- a metal aqueous solution having a concentration of 2.0 M in which nickel sulfate, cobalt sulfate, and manganese sulfate was mixed in a molar ratio of 40:20:40 was prepared, and then the aqueous metal salt solution for forming a core was first introduced into a reactor to form a core.
- an active material having a particle size of 4 to 6 ⁇ m and a tap density of 1.67 g / cc of particles consisting of a core having a constant concentration and a constant shell concentration Prepared.
- a metal solution for forming a core having a concentration of 2.0 M in which nickel sulfate, cobalt sulfate, and manganese sulfate was mixed in a molar ratio of 80:05:15 was prepared, and a shell was formed.
- an aqueous metal salt solution for preparing a 2.0 M metal solution in which nickel sulfate, cobalt sulfate and manganese sulfate were mixed in a molar ratio of 35:20:45 the aqueous metal salt solution for core formation was first introduced into a reactor to form a core.
- the mixing ratio of the aqueous metal salt solution for core formation and the aqueous metal salt solution for shell formation is gradually mixed, mixed at a constant ratio, and introduced at a rate of 0.3 liters / hour to have particle sizes of 4 to 6 ⁇ m and a tap density of 1.73.
- Positive electrode active material for lithium secondary batteries measured in g / cc
- positive electrode active material for lithium secondary batteries measured in particle size of 11 to 14 ⁇ m and tap density of 2.28 g / cc It was produced quality.
- the particles were prepared using a 2.0 M aqueous metal solution in which nickel sulfate, cobalt sulfate, and manganese sulfate were mixed at a 60:20:20 molar ratio.
- An active material having a size of 5 ⁇ m and a tap density of particles of 1.67 g / cc was prepared.
- NCA particles were prepared having a particle size of 3 ⁇ m and constant concentrations of nickel, cobalt and aluminum in the particle.
- LCO particles having a particle size of 2 ⁇ m and a constant cobalt ion concentration were prepared.
- the particles prepared in Preparation Example 5 were mixed with the particles including the shell having a constant core and concentration gradient and the particles prepared in Preparation Examples 1 to 8 as follows, and each tap density, electrode density, and C-rate were mixed.
- the measurement results are shown in Table 1 below.
- the particles having a concentration gradient of the total metal and the particles prepared in Preparation Examples 1 to 8 were mixed as follows and the respective tap density, electrode density, and C-rate were measured. The results are shown in Table 2 below.
- Example 7 the mixing ratio of the active material of Preparation Example 1 having a particle size of 11 ⁇ m and the LCO particles of Preparation Example 8 having a particle size of 2 ⁇ m was mixed as in Table 3 below, and each mixing Particle size analysis (PSA) results and tap densities according to ratios are shown in FIGS. 1 to 2 and Table 3.
- PSA Particle size analysis
- the active material having a concentration gradient prepared in Preparation Example 1 having a particle size of 6 ⁇ m and the active material particles having a concentration gradient prepared in Preparation Example 1 having a particle size of 14 ⁇ m as in Example 10 were mixed and mixed. Post particle size analysis and change in tap density were measured and shown in FIG. 3.
- the active material having a concentration gradient prepared in Preparation Example 1 having a particle size of 6 ⁇ m and the active material particles having a concentration gradient prepared in Preparation Example 2 having a particle size of 12 ⁇ m as in Example 16 were mixed and mixed. After the particle size analysis and the change in the tap density is measured and shown in Figure 4
- the particles having a concentration gradient of two or more concentrations of Mn, Ni, and Co and the particles prepared in Preparation Examples 1 to 8 were mixed as follows, and the respective tap density, electrode density, And C-rate was measured and the results are shown in Table 5 below.
- the positive electrode active material according to the present invention not only enhances the C-rate property but also maintains proper porosity by mixing particles having different sizes and including particles having a gradient of metal ions in the mixed particles. It is possible to prepare a positive electrode active material having a significantly improved density.
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Abstract
La présente invention concerne un matériau actif de cathode pour batteries secondaires au lithium et, plus particulièrement, un matériau actif de cathode pour batteries secondaires au lithium ayant une masse volumique tassée améliorée par mélange de matériaux actifs de cathode ayant différentes tailles l'un par rapport à l'autre comprenant des particules qui ont des densités en gradient en leur sein.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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EP13868086.3A EP2940761B1 (fr) | 2012-12-26 | 2013-12-26 | Matériau actif de cathode pour batteries secondaires au lithium |
CN201380067749.1A CN105009333B (zh) | 2012-12-26 | 2013-12-26 | 用于锂二次电池的正极活性材料 |
US14/652,684 US20150340686A1 (en) | 2012-12-26 | 2013-12-26 | Cathode active material for lithium secondary battery |
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KR20120153025 | 2012-12-26 | ||
KR10-2012-0153025 | 2012-12-26 | ||
KR1020130163942A KR101614991B1 (ko) | 2012-12-26 | 2013-12-26 | 리튬 이차전지용 양극활물질 |
KR10-2013-0163942 | 2013-12-26 |
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WO2014104759A1 true WO2014104759A1 (fr) | 2014-07-03 |
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US (1) | US20150340686A1 (fr) |
EP (1) | EP2940761B1 (fr) |
KR (2) | KR101614991B1 (fr) |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105993090A (zh) * | 2014-10-02 | 2016-10-05 | 艾可普罗有限公司 | 锂二次电池用正极活性材料及包含其的锂二次电池 |
JP2018503238A (ja) * | 2014-12-31 | 2018-02-01 | ベイジン イースプリング マテリアル テクノロジー カンパニー リミテッド | リチウムイオン電池用の傾斜構造を有する多成分材料、その調製方法、リチウムイオン電池の正極及びリチウムイオン電池 |
US20180175388A1 (en) * | 2016-12-16 | 2018-06-21 | Sk Innovation Co., Ltd. | Lithium Secondary Battery |
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CN105993090A (zh) * | 2014-10-02 | 2016-10-05 | 艾可普罗有限公司 | 锂二次电池用正极活性材料及包含其的锂二次电池 |
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JP2018503238A (ja) * | 2014-12-31 | 2018-02-01 | ベイジン イースプリング マテリアル テクノロジー カンパニー リミテッド | リチウムイオン電池用の傾斜構造を有する多成分材料、その調製方法、リチウムイオン電池の正極及びリチウムイオン電池 |
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Also Published As
Publication number | Publication date |
---|---|
KR20140085347A (ko) | 2014-07-07 |
CN105009333A (zh) | 2015-10-28 |
US20150340686A1 (en) | 2015-11-26 |
KR101614991B1 (ko) | 2016-04-22 |
EP2940761A1 (fr) | 2015-11-04 |
EP2940761B1 (fr) | 2019-12-18 |
KR20160049519A (ko) | 2016-05-09 |
CN105009333B (zh) | 2018-04-17 |
EP2940761A4 (fr) | 2016-08-31 |
KR101812517B1 (ko) | 2017-12-28 |
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